CN102951608A - High-volume composite hydrogen storage material, and synthetic method and hydrogen desorption method thereof - Google Patents

High-volume composite hydrogen storage material, and synthetic method and hydrogen desorption method thereof Download PDF

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CN102951608A
CN102951608A CN2011102403060A CN201110240306A CN102951608A CN 102951608 A CN102951608 A CN 102951608A CN 2011102403060 A CN2011102403060 A CN 2011102403060A CN 201110240306 A CN201110240306 A CN 201110240306A CN 102951608 A CN102951608 A CN 102951608A
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陈萍
何腾
熊智涛
吴国涛
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Dalian Institute of Chemical Physics of CAS
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
    • C01B3/06—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents
    • C01B3/065—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents from a hydride
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

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Abstract

The invention relates to a high-volume composite hydrogen storage material, and a synthetic method and a hydrogen desorption method thereof. The composite hydrogen storage material is synthesized through interacting a substance containing H<delta-> with a substance containing H<delta+>, wherein the ratio of the substance containing H<delta-> to the substance containing H<delta+> is 20:1-1:20. Dehydrogenation is carried out through mainly utilizing a thermal decomposition or catalytic thermal decomposition method, wherein the temperature of the thermal decomposition or the catalytic heat dehydrogenation decomposition is 0-300DEG C, and the application amount of a catalyst is 0.01-20mol%.

Description

A kind of high-capacity composite hydrogen storage material and synthetic and put hydrogen methods
Technical field
The present invention relates to hydrogen storage material, specifically a kind of synthetic method of NEW TYPE OF COMPOSITE hydrogen storage material and put hydrogen methods.
Background technology
Hydrogen is pollution-free, renewable with it, the energy advantages of higher is acknowledged as one of substitute energy of future ideality.Yet existing vehicle-mounted hydrogen storage technology for fuel-cell vehicle is difficult to satisfy the needs of practical application, has become one of bottleneck of restriction Hydrogen Energy development.Through effort for many years, the research-and-development activity of hydrogen storage material also makes great progress, and wherein hydroborates gets more and more people's extensive concerning with its high hydrogen richness.For example, lithium borohydride (LiBH 4) and magnesium borohydride (Mg (BH 4) 2) hydrogen content be respectively 18.4wt% and 14.8wt%.But they are extremely stable at normal temperatures and pressures, and to put the hydrogen process be thermo-negative reaction, and hydrogen discharging temperature needs up to more than 300 ℃.Moreover, hydroborate can be followed a kind of gaseous hydride (B harmful to fuel cell in putting the process of hydrogen 2H 6) release, more be unfavorable for the practical application of this material.The recent domestic scholar utilizes LiNH 2, MgH 2, CaH 2Deng material it is carried out chemical modification, slower but these methods still are faced with hydrogen desorption kinetics to obtaining good effect, the problem such as hydrogen discharging temperature is higher.
Recently the researchist finds that the hydrogen discharging temperature of metal borohydride will decrease by forming ammonate.Such as Mg (BH 4) 2(NH 3) 2Can be 150-400 ℃ of release hydrogen; Ca (BH 4) 2(NH 3) 2Can be 250 ℃ of lower release hydrogen; Al (BH 4) 3(NH 3) 6Can be 140-170 ℃ of release hydrogen; Li 2Al (BH 4) 5(NH 3) 6Can be 130 ℃ of lower release hydrogen.In above-mentioned bibliographical information, they think BH 4In H δ-Same NH 3In H δ+Interact and cause the material dehydrogenation, therefore reduced the hydrogen discharging temperature of hydroborate.Based on this, we attempt to seek a kind of H of containing δ+Material by with contain H δ-Material (such as hydroborate, metal hydride, alanate etc.) be combined into a kind of novel hydrogen storage material, can under mild conditions, discharge the hydrogen of appreciable amount.
Hydrazine (NH 2NH 2) a kind of liquid at room temperature, have high hydrogen richness (12.5wt.%).Because the H in the hydrazine links to each other with the N element, therefore, H is all with part positive charge.It may with contain H δ-Material cladding form a kind of hydrogen storage material.
Summary of the invention
In order to seek with H δ+And H δ-Be the synthetic method of the hydrogen storage material on basis, and further reduce hydrogen discharging temperature, the present invention adopt hydroborate, alanate, metal hydride be equal to organic derivative, the hydrazine of hydrazine, hydrazine metal derivative, contain-NH 2The organism of group etc. interact and synthesize storage hydrogen novel material, and further reduce hydrogen discharging temperature by adding cheap catalyzer.
For achieving the above object, the present invention is by the following technical solutions:
A kind of high-capacity composite hydrogen storage material is mainly by containing H δ-Material with contain H δ+Matter interaction and synthesize, contain H δ-Material and contain H δ+Mol ratio between the material is between 100: 1 to 1: 100.
Contain H δ-Material and contain H δ+Mol ratio between the material is between 20: 1 to 1: 20.
Contain H δ-Material be in hydroborate, alanate, the metal hydride one or two or more kinds; Preferably hydroborate contains H δ-Material be in the hydroborate one or two or more kinds;
Contain H δ+Material be organic derivative, the hydrazine of hydrazine, hydrazine metal derivative, contain-NH 2In the organism of group one or two or more kinds; Be preferably hydrazine or contain-NH 2The organism of group contains H δ+Material be hydrazine or contain-NH 2In the organism of group one or two or more kinds.
The organic derivative molecular formula of described hydrazine is RHNNHR ', wherein R and R ' be respectively-Me ,-Cy ,-Pr ,-Ph or-a kind of in the Et organic group;
The metal derivative molecular formula of described hydrazine is M (HNNH 2) n, wherein M is a kind of among Li, Na, K, Mg, the Ca, n is the valency 1 or 2 of M.
Synthesizing of described hydrogen storage material: under inert atmosphere, contain H δ-Material with contain H δ+Material by the synthetic hydrogen storage material of mutual coordination, building-up process adopts ball milled, mixes method or steam adsorption method.
Material therefor is the material of high hydrogen richness, and therefore operation must operate under inert atmosphere, for example N 2Or in the glove box of Ar filling.
Described hydrogen storage material put hydrogen methods, adopt the airtight or open hydrogen system of putting, be preferably in closed system and transfer hydrogen; Put the hydrogen service temperature between-100 ℃ to 600 ℃, be preferably between 0 ℃ to 300 ℃; Method of dehydrogenating mainly comprises thermolysis or Catalytic Thermal Decomposition.
Composite hydrogen storage material further reduces hydrogen discharging temperature by adding catalyzer.
In the Catalytic Thermal Decomposition process, catalyzer by in transition metal, transition metal salt or the alloy one or two or more kinds;
Transition metal be in IB, IIB, IIIB, IVB, VB, VIB, VIIB or the VIIIB family element in one or two or more kinds; The salt of transition metal is organic metal salt, the Cl of above-mentioned transition metal -, SO 4 2-, NO 3 -, NO 2 -, F -, Br -Or PO 4 3-Salt in one or two or more kinds;
Alloy is two yuan or the multicomponent alloy that forms between Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Rh, Pd, Ag, Ir, Pt or the Au, or two yuan or multicomponent alloy of one or more formation among one or more and P, C, B or the N among Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Rh, Pd, Ag, Ir, Pt or the Au; Be preferably the alloy that forms between a kind of transition metal and B, N or the C.
Transition metal is preferably among Fe, Co, Ni, Cu, Ru, Rh, Pd, Ag, Pt or the Au one or two or more kinds; The salt of transition metal is preferably organic metal salt, the Cl of above-mentioned transition metal -, SO 4 2-, NO 3 -, NO 2 -, F -, Br -Or PO 4 3-Salt in one or two or more kinds;
Alloy is the alloy that forms between a kind of and B, N among Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Rh, Pd, Ag, Ir, Pt, the Au or the C.
The consumption of described catalyzer is between the 0.01mol% to 20mol% of composite hydrogen storage material.
The addition means in the composite hydrogen storage material of described catalyzer can adopt with composite hydrogen storage material and jointly carry out ball milled, mixes method or liquid coprecipitation method.
The present invention has following advantage:
1. this hydrogen storage material has been because adopted hydroborate, and the higher material of the hydrogen contents such as hydrazine is as reactant, therefore the overall hydrogen content of this system is higher.
2. this system is mainly utilized the method synthetic samples such as ball milled, paddling process, and synthesis technique is simple.
3. pure hydroborate reaction hydrogen discharging temperature generally needs greater than 300 ℃, and this hydroborate-hydrazine compound system has reduced the hydroborate hydrogen discharging temperature effectively, for example FeCl 3The LiBH that modifies 4-NH 2NH 2Can transfer hydrogen at 140 ℃.
4. the heat decomposition temperature of pure hydrazine is about 180 ℃, and the decomposition primary product is N 2And NH 3, the selectivity of hydrogen is almost nil.Even there is noble metal catalyst to exist, below 300 ℃, the selectivity of hydrogen is very low (being lower than 10%) also.And degradation production has suppressed NH in hydroborate-hydrazine compound system 3Generation, and the selectivity of hydrogen is at a lower temperature near 100%.
Description of drawings
Fig. 1, pure LiBH 4And LiBH 4-NH 2NH 2The XRD spectra of mixture.
Fig. 2, under 150 ℃, 5.0mo l%FeCl 3The LiBH that mixes 4-NH 2NH 2Hydrogen desorption isotherms.
Fig. 3, Mg (BH 4) 2The reactor schematic diagram of absorption hydrazine.
Fig. 4, under 250 ℃, Mg (BH 4) 2-2NH 2NH 2Hydrogen desorption isotherms.
Fig. 5, LiH and NH 2NH 2The XRD spectra of reaction product.
Fig. 6, NaBH 4-NH 2NH 2The XRD spectra of mixture.
Fig. 7, LiBH 4-2NH 2NH 2The XRD spectra of mixture.
Fig. 8,2LiBH 4-1NH 2NH 2The XRD spectra of mixture.
Embodiment
Embodiment 1
1.LiBH 4-NH 2NH 2The preparation of mixture
In glove box, take by weighing the lithium borohydride of 361.8mg, measure simultaneously the hydrazine of 0.5ml, two kinds of samples are put into same ball grinder.Note, this moment, two kinds of samples can not contact.After this ball grinder sealing, carefully be transferred on the ball mill, under the 150rpm rotating speed, ball milling 2 hours.After ball milling finished, the ball grinder internal pressure was unchanged, and made sample is solid.Fig. 1 is X-ray diffraction (XRD) spectrogram of made sample, can find out, with pure LiBH 4Compare LiBH 4-NH 2NH 2Mixture has formed new species, is different from LiBH fully 4
2. the adding of catalyzer
In glove box, take by weighing the LiBH of 500mg 4-NH 2NH 2Mixture takes by weighing the FeCl of 77.6mg simultaneously 3, two kinds of samples are put into same ball grinder.After this ball grinder sealing, carefully be transferred on the ball mill, under the 150rpm rotating speed, ball milling 5 hours can make 5.0mol%FeCl 3The LiBH that mixes 4-NH 2NH 2FeCl 3In mechanical milling process, by LiBH 4-NH 2NH 2In-situ reducing is that the Fe of lower valency is catalyst based.
3. dehydrogenation reaction
Take by weighing 5%FeCl 3Doped LiBH 4-NH 2NH 2Sample 100mg from room temperature, with 2 ℃/min temperature programming to 150 ℃, finishes in 150 ℃ of lower constant temperature to reaction in airtight reactor tube.As shown in Figure 2, record this system hydrogen desorption capacity and be about 3.8equi v.H 2/ LiBH 4, be equivalent to 14.1wt%H 2/ LiBH 4-NH 2NH 2
Embodiment 2
1.Mg (BH 4) 2-2NH 2NH 2The preparation of mixture
In glove box, take by weighing the self-control Mg (BH of 444.1mg 4) 2, measure simultaneously the hydrazine of 0.5ml, two kinds of samples are put into the position of encloses container indicating as shown in Figure 3, do not contact mutually.Utilize the vapour pressure of hydrazine, Mg (BH 4) 2Hydrazine can be adsorbed onto in the solid phase fully, form Mg (BH 4) 2-2NH 2NH 2Mixture.Sample Mg (BH 4) 2-2NH 2NH 2Must in enclosed system, wear out for 1 week.
2. dehydrogenation reaction
Take by weighing Mg (BH 4) 2-2NH 2NH 2Sample 100mg from room temperature, with 2 ℃/min temperature programming to 250 ℃, finishes in 250 ℃ of lower constant temperature to reaction in airtight reactor tube.As shown in Figure 4, record this system hydrogen desorption capacity and be about 7.6equiv.H 2/ Mg (BH 4) 2, be equivalent to 12.8wt%H 2/ Mg (BH 4) 2-2NH 2NH 2
Embodiment 3
LiH-NH 2NH 2Preparation
In glove box, take by weighing the lithium hydride of 128.9mg, measure simultaneously the hydrazine of 0.5ml, two kinds of samples are put into same ball grinder.Note, this moment, two kinds of samples can not contact.After this ball grinder sealing, carefully be transferred on the ball mill, under the 150rpm rotating speed, ball milling 2 hours.After ball milling finished, the gas that utilizes mass spectrum to record in the ball grinder was hydrogen, and pressure change is 1mol H 2/ LiH, and made sample is solid.Fig. 5 is X-ray diffraction (XRD) spectrogram of made sample, can find out, compares LiH and NH with pure LiH 2NH 2Reaction has generated new species, is different from LiH fully.
Embodiment 4
NaBH 4-NH 2NH 2The preparation of mixture
In glove box, take by weighing the sodium borohydride of 593.8mg, measure simultaneously the hydrazine of 0.5ml, two kinds of samples are put into same ball grinder.Note, this moment, two kinds of samples can not contact.After this ball grinder sealing, carefully be transferred on the ball mill, under the 150rpm rotating speed, ball milling 2 hours.After ball milling finished, the gaseous tension that records in the ball grinder was unchanged, and made sample is solid.Fig. 6 is X-ray diffraction (XRD) spectrogram of made sample, can find out, with pure LiBH 4Compare LiBH 4-NH 2NH 2Mixture has formed new species, is different from NaBH fully 4
Embodiment 5
LiBH 4-2NH 2NH 2The preparation of mixture
In glove box, take by weighing the lithium borohydride of 180.9mg, measure simultaneously the hydrazine of 0.5ml, two kinds of samples are put into same ball grinder.Note, this moment, two kinds of samples can not contact.After this ball grinder sealing, carefully be transferred on the ball mill, under the 150rpm rotating speed, ball milling 2 hours.After ball milling finished, the ball grinder internal pressure was unchanged, and made sample is solid.Fig. 7 is X-ray diffraction (XRD) spectrogram of made sample, can find out, with pure LiBH 4Compare LiBH 4-2NH 2NH 2Mixture has formed new species, is different from LiBH fully 4
Embodiment 6
2LiBH 4-1NH 2NH 2The preparation of mixture
In glove box, take by weighing the lithium borohydride of 723.6mg, measure simultaneously the hydrazine of 0.5ml, two kinds of samples are put into same ball grinder.Note, this moment, two kinds of samples can not contact.After this ball grinder sealing, carefully be transferred on the ball mill, under the 150rpm rotating speed, ball milling 2 hours.After ball milling finished, the ball grinder internal pressure was unchanged, and made sample is solid.Fig. 8 is X-ray diffraction (XRD) spectrogram of made sample, can find out, with pure LiBH 4Compare 2LiBH 4-1NH 2NH 2Mixture has formed new species, is different from LiBH fully 4

Claims (11)

1. high-capacity composite hydrogen storage material is characterized in that:
Described hydrogen storage material mainly by contain H δ-material with contain H δ+matter interaction and synthesize, contain H δ-material and the mol ratio that contains between H δ+material is between 100: 1 to 1: 100.
2. according to the described hydrogen storage material of claim 1, it is characterized in that:
The mol ratio that contains H δ-material and contain between H δ+material is between 20: 1 to 1: 20.
3. according to the described hydrogen storage material of claim 1, it is characterized in that:
Contain H δ-material be in hydroborate, alanate, the metal hydride one or two or more kinds;
Contain H δ+material be organic derivative, the hydrazine of hydrazine, hydrazine metal derivative, contain-in the organism of NH2 group one or two or more kinds.
4. according to the described hydrogen storage material of claim 3, it is characterized in that:
The organic derivative molecular formula of described hydrazine is RHNNHR ', wherein R and R ' be respectively-Me ,-Cy ,-Pr ,-Ph or-a kind of in the Et organic group;
The metal derivative molecular formula of described hydrazine is M (HNNH2) n, and wherein M is a kind of among Li, Na, K, Mg, the Ca, and n is the valency 1 or 2 of M.
5. according to the described hydrogen storage material of claim 1, it is characterized in that:
Contain H δ-material be in the hydroborate one or two or more kinds;
Contain H δ+material be hydrazine or contain-in the organism of NH2 group one or two or more kinds.
6. the synthetic method of the described hydrogen storage material of claim 1, it is characterized in that: under inert atmosphere, contain H δ-material with contain H δ+material by H δ-with the synthetic hydrogen storage material of coordination of H δ+mutually, building-up process employing ball milled, mix method or steam adsorption method.
The described hydrogen storage material of claim 1 put hydrogen methods, it is characterized in that: adopt the airtight or open hydrogen system of putting, be preferably in closed system and transfer hydrogen; Put the hydrogen service temperature between-100 ℃ to 600 ℃, be preferably between 0 ℃ to 300 ℃; Method of dehydrogenating mainly comprises thermolysis or Catalytic Thermal Decomposition.
8. according to the hydrogen methods of putting claimed in claim 7, it is characterized in that: in the Catalytic Thermal Decomposition process, catalyzer by in transition metal, transition metal salt or the alloy one or two or more kinds; Transition metal be in IB, IIB, IIIB, IVB, VB, VIB, VIIB or the VIIIB family element in one or two or more kinds;
The salt of transition metal be above-mentioned transition metal organic metal salt, Cl-, SO42-, NO3-, NO2-, F-, Br-or PO43-, salt in one or two or more kinds;
Alloy is two yuan or the multicomponent alloy that forms between Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Rh, Pd, Ag, Ir, Pt or the Au, or two yuan or multicomponent alloy of one or more formation among one or more and P, C, B or the N among Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Rh, Pd, Ag, Ir, Pt or the Au; Be preferably the alloy that forms between a kind of transition metal and B, N or the C.
9. according to the hydrogen methods of putting claimed in claim 8, it is characterized in that: described
Transition metal is among Fe, Co, Ni, Cu, Ru, Rh, Pd, Ag, Pt or the Au one or two or more kinds;
The salt of transition metal be above-mentioned transition metal organic metal salt, Cl-, SO42-, NO3-, NO2-, F-, Br-or PO43-, salt in one or two or more kinds;
Alloy is the alloy that forms between a kind of and B, N among Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Rh, Pd, Ag, Ir, Pt, the Au or the C.
10. according to the hydrogen methods of putting claimed in claim 8, it is characterized in that: the consumption of described catalyzer is between the 0.01mol% to 20mol% of composite hydrogen storage material.
11. according to the hydrogen methods of putting claimed in claim 8, it is characterized in that: the addition means in the composite hydrogen storage material of described catalyzer can adopt with composite hydrogen storage material and jointly carry out ball milled, mixes method or liquid coprecipitation method.
CN2011102403060A 2011-08-19 2011-08-19 High-volume composite hydrogen storage material, and synthetic method and hydrogen desorption method thereof Pending CN102951608A (en)

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